Process of purifying sugar.



UNITED STATES Patented December 15, 1903.

PATENT OFFICE.

CLAUS A. SPRECKELS ANDCHARLES A. KERN, OF NEW YORK, N. Y.,

ASSIGNORS TO FEDERAL SUGAR REFINING COMPANY, OF JERSEY CITY, NEW JERSEY, A CORPORATION OF NEW JERSEY.

PROCESS OF PURIFYING SUGAR.

SPECIFICATION formingpart of Letters Patent No. 746,891, dated December 15, 1903.

Application filed July 2, 1902. Serial No. 114,033. (No specimens.)

To all whom it may concern.-

Be it known that we, CLAUS A. SPREOKELS and CHARLES A. KERN, citizens of the United States, and residents of the borough of Manhattan, city and State of New York, have invented certain new and useful Improvements in Processes of Purifying Sugar and Solutions Thereof, of which the following is a full and true description.

The object of this invention is to. economically and quickly remove impurities from sugar or sugar solutions.

The present invention isa specific form of the process described and claimed in our Letters Patent of the United States N 0. 698,150, dated April 22, 1902, for processes of purifying sugar and solutions thereof. That patent covers, broadly, the employment of a sulfonated fluid defecating or cleansing agent for the treatment of impure sugar.

We have ascertained that there are certain advantages hereinafter recited resulting from the employment of a fatty sulfonated or sulfooleaginous defecating or cleansing agent, viz: one consisting of or containing a cleanser produced by the action of sulfuric acid upon fats, fatty oils, or fatty acids in such proportions that there is no injurious efiect upon the sugar from the solfuric acid and bodies are produced which have greater absorbent properties for the earthy or metallic salts and for the invert sugar ordinarily found associated with sugar or' sugar-bearing bodies and caramel produced in the process of manufacture than the adherent properties of such impurities to the sugar itself, and subsequently separating the sugar from the defecating or cleansing composition containing the absorbed impurities.

lVe believe we are the first to discover the use of fatty sulfonated or suifooleaginous bodies or material containing the same for the purpose of cleansing or purifying sugar.

In our said patent we have substantially stated as an example of the way in which our cleansing material may be prepared for use the following: Mix sulfuric acid, preferably of 1.835 specific gravity, (66 Baum,) in the proportion of, say, fifty parts, by weight, of

acid with onehundred parts, by weight, of one or more fats, fatty oils, and fatty acids. The sulfuric acid is added to the body or bodies gradually or at all events under such conditions that a low temperature will bemaintained, the work being preferably carried out in a cooled receptacle, and the mixture is allowed to stand for a few hours. The excess of acid is removed or neutralized either by the addition of alkali or by the addition of water or gravital separation. The proportion and strength of acid above suggested may be used in sulfonating each and every one of the substances or mixtures hereinafter mentioned. The cleansing or defecating body produced is of course in all cases fluid. The proportion and strength of acid may of course be varied in well-known ways and other well-known acids may be mixed with the sulfuric acid without departure from our invention, it being borne in mind that the result is that the body when acted upon by the sulfuric acid and in the condition in which it is to be used will not contain sulfuric acid in any amount injurious to the sugar and will have an absorbent property for the impurities greater than the adherent properties of such impurities for the sugar itself.

As recommended in our patents, we may in preparing a fatty sulfonated or sulfodla' aginous body proceed as follows: Take two parts, by weight, of a fattyoil, refined cotton-seed oil being an example, and add while stirring the oil one part, by weight, of suifuric acid, (preferably 66 Baum,) preferably mixing the acid with the oil gradually, so as to maintain a low temperature. After the incorporation of the acid allow the mixture to stand for a few hours and then preferably remove or neutralize the excess of acid in the mixture. For this purpose we may neutralize the mixture by the addition of an alkali or mixture of alkalies, preferably carbonate of soda,causti c soda, carbonate of potash, causticpotash, or combinations thereof. When not neutralizing by the use of alkali, we proceed as folio ws: Add water about equal tothe amount of oil in the'original mixture and mix thoroughly. On standing the mixture separates into two layers, the upper fluid layer being the material in course of treatment and the lower consisting of water containing the surplus acid and other useless products, and we leave the mixture standing for several hours in a vessel properly arranged and then draw off the water containing superfluous acid, 850. To the mixture obtained by the addition of alkalies, as above described, or by the addition of water, as above described, add a solution of common salt and water to free the mixture from any remaining acid or water, or excess of alkali when used. After each addition of salt and water we allow the mixture to settle and draw off the saline solution. When the mixture is practically free from water or from excess of alkali, when used, we may, as described in an application, Serial No. 82,825, filed by us on November 19, 1901, mix the fatty sulfonated or sulfooleaginous body with or dissolve it in kerosene-oil or other hydrocarbon oil or a mixture containing hydrocarbon oil. v

A fatty sulfonated or sulfooleaginous body dissolved in or mixed with a hydrocarbon oil or hydrocarbon-oil mixture, has distinct beneficial characteristics and properties for the purpose of defecating or cleansing sugar, and we believe it to be a composition new in the arts.

When employing alkali to neutralize the acid, we have obtained good results by employing one part of caustic soda to each fifteen parts of the modified mixture.

We have obtained good results by adding about fifty per cent. of kerosene-oil; but we do not state this as a fixed percentage, since it may be materially varied.

The use of an alkali, above described, for the purpose of neutralizing free sulfuric acid may result, as is well understood, in the production of sulfonic-acid salts or closely allied salts in the defecating or cleansing liquid; but such salts so made are included by us under the generaldesignation of bodies included under our invention.

The following are fats or fatty bodies which we have tested and found to be acted upon and to act in the manner described, viz: olive-oil, castor-oil, cotton-seed oil, cocoanutoil, linseed-oil, rape-oil, peanut-oil, lard, tallow, cod-liver oil, fish-oil, (Menhaden oil,) lard-oil, oleic acid; but all of the substances above named are given as examples only of our invention.

Our invention also includes the employment of defe cating or cleansing liquids containing sulfonated or sulfooleaginous bodies made by utilizing mixtures containing one or more fats or fatty bodies. We have attained good results from a considerable number of such mixtures.

As the fats are solid oils and as the fatty acids, as is well known, have oily or greasy characteristics and as all of the above substances are acted upon by sulfuric acid in the manner described and also when sulfonated act upon sugar and its impurities in analogous and equivalent ways, We hereinafter include them all under the generic term fatty oleaginous bodies and when acted on by sulfuric acid in the manner described we term the derivativesfattysulfooleaginous bodies. All the derivative cleansing agents mentioned are properly included also under the term fatty sulfonated bodies, whether properly and strictly called oleaginous or not.

Many forms of sulfooleaginous bodies are well known in the arts for other purposes,and hence a more particular description of the methods of producing the same is not required. I

The amount of the composition used may be varied to suit the difierent qualities of the material being treated; but the mass of sugar-bearing material and cleanser should be semifluid, at least, if not already so. In all cases there should of course be enough to absorb out the impurities. For example, We have obtained excellent results when treating raw sugar by employing eight pounds of cleanser to each ten pounds of raw sugar. As the fatty sulfonated cleanser has no inju rious effect upon the sugar-crystals or sugar liquor, the quantity of composition may be increased as desired.

We have found that the employment of a fatty sulfonated defecating or cleansing agent for the treatment of sugar or sugar solutions is advantageous.

As stated in our said Patent No. 698,150, our preferred method of separating a sulfonated or sulfooleaginous body and impurities from sugar-crystals is as follows: After the intimate mixture of the cleansing material in liquid form and the sugar under treatment we preferably employ a centrifugal machine driven at a high rate of speed for the purpose of separation. The mixture of the composition and the material being treated is put into the centrifugal machine and the composition and the absorbed impurities are expelled from the mass. This expelled mixture may subsequently be treated for the recovery therefrom of the cleanser. The mechanical impurities, if any-such as sticks, stoues,straws, &cstill left with the sugar after separating out the composition and the impurities it has absorbed may be removed in any well-known manner, as by dissolving the mass of sugar-crystals in water and by the filtration hereinafter described. In order to remove any slight traces of our cleansing body or composition from a mass of sugarcrystals, we may subject the mass to a further treatment, as by dissolving the same, adding fullers earth or a substitute therefor, and then filtering out the same and crystallizing the sugar.

If the material to be treated is in the form of sugar-juice, sugar liquor, or molasses, we may mix the same with an amount of fatty sulfonated or sulfooleaginous body approximately equal in amount to the weight of the impurities, as ascertained by chemical analysis of a portion of the liquor, contained in the liquor in order to absorb out the impurites other than the solid impurities, and We then subject the mixture to any desired subsequent processes for filtering out the purified sugar liquor, as by the use of fullers earth, above described by us, and for subsequent crystallization of the sugar.

If thesolution is at all acid, it may be neutralized by the addition of a little slaked lime.

If any of the fatty sulfonated or sulfooleagiuous bodies utilized are in the form used at all soluble in Water they may nevertheless be readily availed of in connection with concentrated sugar solutions, as they are practically insoluble in such sugar solutions.

The above or any particular process for separating the fatty-sulfonated or sulfooleaginous cleanser from the sugar is, however, not an essential part of our generic invention, but forms ofprocess for removing the cleansing-body are more fully described in separate Patents Nos. 669,933 and 700,099, dated May 13, 1902.

We claim- 1. In the method of cleansing sugar from its impurities, the step which consists in mixing with the impure sugar a cleansing agent pure sugar, a cleansing agent containing a snlfonated fatty body, and then separating the cleansing agent and the impurities carried by it, from the sugar, substantially as described. I

5. In the method of cleansing sugar from its impurities, the step consisting in mixing with the impure sugar a cleansing agent containing a snlfonated fatty body mixed with hydrocarbon oil, substantially as described.

CLAUS A. SPBEOKELS. CHARLES A. KERN.

Witnesses:

TEILE H. MiiLLER, STEPHEN E'ren. 

